CN104280308A - Method for measuring content of carbon black in technical gas - Google Patents
Method for measuring content of carbon black in technical gas Download PDFInfo
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- CN104280308A CN104280308A CN201410523002.9A CN201410523002A CN104280308A CN 104280308 A CN104280308 A CN 104280308A CN 201410523002 A CN201410523002 A CN 201410523002A CN 104280308 A CN104280308 A CN 104280308A
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Abstract
The invention discloses a method for measuring the content of carbon black in technical gas. The measurement method comprises the steps of preparing technical gas to be measured from technical gas containing carbon black; feeding the technical gas to be measured into carbon black adsorption liquid to obtain carbon black enrichment liquid and wet technical gas which does not contain carbon black; obtaining the carbon black in the carbon black enrichment liquid, and weighing dry carbon black; and calculating a ratio of the weight of the dry carbon black to the volume of the technical gas to be measured to obtain the content of the carbon black in the technical gas. The carbon black is gathered into the carbon black adsorption liquid to realize separation of the carbon black in the technical gas to be measured from the technical gas, and the content of the carbon black in the technical gas can be measured by a weight method; a relative error introduced by the measurement method is relatively small, and the measured content of the carbon black in the technical gas is relatively accurate, and therefore, the content of the carbon black can be monitored in real time, and the influence caused by subsequent technical production is avoided.
Description
Technical field
The present invention relates to coal chemical technology, the assay method of content of carbon black in a kind of process gas.
Background technology
Carbon black refers to hydro carbons black powder material through gas phase rough burning or pyrolysis under the strict process conditions controlled.Its composition mainly elemental carbon, and containing a small amount of oxygen, hydrogen and sulphur etc.Carbon black particle almost spherical, particle diameter is between 10 ~ 500 μm.The usually clinkering or be agglomerated into the dendritic or fibrilla aggregates of three-dimensional key of many particles.
Many factories gasification furnace, in coal-water slurry combustion, insufficiently can produce certain carbon black owing to burning.Can a part be removed although follow-up through washing filtering, in actual production process, need the content of carbon black to producing to control, impacting in order to avoid produce subsequent technique.During the too high levels of carbon black, not only can block the pipeline of synthetic gas on-line analysis instrument, damage is caused to parts such as the detecting device of instrument and chromatographic columns, when the carbon black that content is too high simultaneously progressively enters follow-up conversion and clean unit, the operation of follow-up equipment is impacted.Therefore need to monitor the content of carbon black and measure in actual production.
Current existing method mainly contains two kinds, and a kind of is the smoke density experimental method (ASTMD of the external color contrast adopted
2156-65), another is burning absorption titrimetry (1988Vol17No3, oil and gas chemical industry) of Natural Gas Research Inst., Sichuan Petroleum Bureau's invention.
After external smoke density experimental method refers to and get oxygen filtration under specified requirements, filter paper and ten standard color range color boards are compared, the method can determine the grade of content of carbon black, but cannot determine concrete containing numerical quantity, and when foreign pigment exists, also can measure chromatmetry and have certain influence.
It is by being filtered out by the carbon black in gas that the burning of Natural Gas Research Inst., Sichuan Petroleum Bureau absorbs titrimetry, and then in oxygen stream, burning makes generation CO
2, determine the growing amount of carbon black with the assay method of the absorption of excessive hydrogen baryta, oxalic acid standard solution residual titration.Although this burning absorbs the concrete content that titrimetry can determine carbon black, but in experimentation, need burner to be also placed in scene, and follow-up needs absorbs a series of programs such as titration, both do not meet the requirement of Analysis of industrialized production, easily introduced personal error simultaneously.In addition, because the sulfur content in gasification synthesis gas is higher, also comparatively large on the impact of burning absorption process, therefore burning absorption titrimetry can not meet simple in time to the analysis requirement of content of carbon black.
Therefore, the assay method of the content of carbon black in above-mentioned similar gasification synthesis technique gas is still had much room for improvement.
Summary of the invention
The present invention aims to provide a kind of assay method of content of carbon black, cannot the relatively simple deficiency measuring content of carbon black in process gas exactly in prior art to improve.
To achieve these goals, according to an aspect of the present invention, provide the assay method of content of carbon black in a kind of process gas, this assay method comprises the following steps: get the process gas containing carbon black, forms process gas to be measured; Process gas to be measured is passed in carbon black adsorption liquid, obtains carbon black pregnant solution and not containing the moist process gas of carbon black; Obtain the carbon black in carbon black pregnant solution, and weigh the quality of dry carbon black; Calculate the ratio between the quality of dry carbon black and process gas volume to be measured, obtain the content of carbon black in process gas.
Further, the volume of above-mentioned process gas to be measured is calculated by following steps: the moist process gas not containing carbon black is passed into wet test meter by (1), calculate 0 DEG C according to formula I, the volume V1 of process gas dry under 1 atmospheric pressure, formula I is as follows:
In formula I: the unit of V1 is Nm
3, A be by wet test meter not containing the gas flow of moist process gas of carbon black, P is the pressure of wet test meter, water saturation vapour pressure when being t DEG C that PW is temperature, and t is the temperature value that wet test meter reads;
(2) calculate the water vapor that is dissolved in carbon black pregnant solution at 0 DEG C according to formula II, the condensate water volume V2 under 1 atmospheric pressure, formula II is as follows:
In formula II: the unit of V2 is Nm
3, C is the quality of carbon black pregnant solution relative to the increase of carbon black adsorption liquid, and B is the quality of dry carbon black, and 18 is the molecular weight of water, and 22.4 is 273K, under 1 atmospheric pressure, and the volume of 1mol water vapor;
(3) calculate V1 and V2 add and, obtain process gas volume to be measured.
Further, process gas to be measured is passed in the step obtaining carbon black pregnant solution in carbon black adsorption liquid, carbon black adsorption liquid is placed on respectively at least two absorption bottles, and by process gas to be measured successively by each absorption bottle, collect in each absorption bottle the step of carrying out the carbon black obtained in carbon black pregnant solution after carbon black pregnant solution.
Further, in each absorption bottle, the volume of carbon black adsorption liquid is not less than 10% of absorption bottle volume, and process gas passes into 1.5cm to carbon black adsorption liquid liquid level; Preferably, absorption bottle is 2 ~ 6, and the volume of absorption bottle is 250ml-1000ml, and the carbon black adsorption liquid in absorption bottle is no less than 100ml; Preferred carbon black adsorption liquid is water, is more preferably ultrapure water.
Further, process gas to be measured passed in carbon black adsorption liquid, obtain in the step of carbon black pregnant solution, regulate process gas to be measured to pass into flow velocity in carbon black adsorption liquid, the speed making process gas to be measured produce bubble in carbon black adsorption liquid is 2 ~ 3/min.
Further, obtain the carbon black in carbon black pregnant solution, and the step measuring the quality of dry carbon black comprises: S1, get filtering material, measure the quality a of filtering material before absorbing; S2, carbon black pregnant solution to be filtered by filtering material, after drying, measure the quality b of filtering material after absorption; Difference between S3, the quality b calculating the rear filtering material of absorption and the quality a absorbing front filtering material, obtains the quality of dry carbon black.
Further, in above-mentioned steps S1, get filtering material, filtering material is immersed in carbon black adsorption liquid, after taking out drying, measure the quality a of filtering material before absorbing.
Further, in above-mentioned steps S2, drying condition is at 105 ~ 115 DEG C, dries 2 ~ 4h.
Further, in above-mentioned steps S2, N/mono-getting carbon black pregnant solution cumulative volume is filtered by filtering material, measures the quality b of the rear filtering material of absorption after drying; In step S3, the quality of dry carbon black is N times of the difference between the quality b of filtering material after absorption and the quality a absorbing front filtering material.
Further, in above-mentioned steps S2, carbon black pregnant solution is at least iterated through filtering material and carry out filtration step 3 times, preferably 3 ~ 5 times.
Further, above-mentioned filtering material is included in the filter paper filtering and first contact with carbon black pregnant solution in carbon black pregnant solution process, and is positioned at the acid-washed asbestos below filter paper; Preferred filter paper is quantitative filter paper.
Further, in above-mentioned filtration step, filtering material is placed in Buchner funnel or glass sand core funnel filters, the diameter of preferred Buchner funnel or glass sand core funnel is not more than 10cm; The diameter of the filter paper and acid-washed asbestos that are more preferably arranged in Buchner funnel or glass sand core funnel is not more than 11cm.
Further, before the moist process gas not containing carbon black is passed into wet test meter by above-mentioned steps (1), also comprise and will not contain the step of moist process gas by the sour gas in the moist process gas of alkaline solution absorption of carbon black; Preferred alkaline solution to be mass concentration be 0.3 ~ 0.8% alkaline solution, more preferably mass concentration is the alkaline solution of 0.5%; Preferred alkaline solution is NaOH, KOH, NaHCO
3or KHCO
3solution.
Further, after the step of above-mentioned absorption sour gas, step (1) further comprises and the moist process gas removing sour gas is passed into the CaCl that mass concentration is 0.3 ~ 0.8% before the moist process gas not containing carbon black is passed into wet test meter
2solution absorbs the step of ammonia, preferred CaCl
2solution to be mass concentration be 0.5% CaCl
2solution.
Apply technical scheme of the present invention, be separated with process gas to be applied by the carbon black in process gas to be measured being trapped in carbon black adsorption liquid the solid impurity carbon black realized in process gas to be measured, then respectively by the volume of the quality and process gas to be measured that measure carbon black in carbon black pregnant solution, the content of carbon black in process gas to be measured can just be obtained.The advantage of this assay method of the present invention is the trapping work that directly can complete carbon black in production scene, then in laboratory, completes filtration, the dry work with weighing.Due to the present invention's colourimetry compared to existing technology and combustion titration method, what adopt is that mass method is to measure the content of carbon black in process gas, therefore the relative error introduced is also less, in the process gas recorded, the content of carbon black is relatively more accurate, thus can monitor in real time the content of carbon black, avoid producing subsequent technique impacting.
Accompanying drawing explanation
The Figure of description forming a application's part is used to provide a further understanding of the present invention, and schematic description and description of the present invention, for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 shows the process chart of content of carbon black in the mensuration process gas provided in a kind of typical embodiment of the present invention.
Embodiment
It should be noted that, when not conflicting, the embodiment in the application and the feature in embodiment can combine mutually.Below with reference to the accompanying drawings and describe the present invention in detail in conjunction with the embodiments.
In the typical embodiment of one of the present invention, provide the assay method of content of carbon black in a kind of process gas, this assay method comprises the following steps: get the process gas containing carbon black, forms process gas to be measured; Process gas to be measured is passed in carbon black adsorption liquid, obtains carbon black pregnant solution and not containing the moist process gas of carbon black; Obtain the carbon black in carbon black pregnant solution, and weigh the quality of dry carbon black; Calculate the ratio between the quality of dry carbon black and process gas volume to be measured, obtain the content of carbon black in process gas.
Said determination method of the present invention, be separated with process gas to be applied by the carbon black in process gas to be measured being trapped in carbon black adsorption liquid the solid impurity carbon black realized in process gas to be measured, then respectively by the volume of the quality and process gas to be measured that measure carbon black in carbon black pregnant solution, the content of carbon black in process gas to be measured can just be obtained.The advantage of this assay method of the present invention is the trapping work that directly can complete carbon black in production scene, then in laboratory, completes filtration, the dry work with weighing.Due to the present invention's colourimetry compared to existing technology and combustion titration method, what adopt is that mass method is to measure the content of carbon black in process gas, therefore the relative error introduced is also less, in the process gas recorded, the content of carbon black is relatively more accurate, thus can monitor in real time the content of carbon black, avoid producing subsequent technique impacting.
In said determination method of the present invention, the measure method long-pending to process gas to be measured there is no particular/special requirement, as long as the content of carbon black in process gas to be measured does not block the pipeline of gauging instrument, any method that can measure process gas volume to be measured is all applicable to the present invention.In a kind of preferred embodiment of the present invention, above-mentioned process gas volume to be measured adopts following methods to calculate:
(1) the moist process gas not containing carbon black is passed into wet test meter, calculate 0 DEG C according to formula I, the volume V1 of process gas dry under 1 atmospheric pressure, formula I is as follows:
In above-mentioned formula I: the unit of V1 is Nm
3, A be by wet test meter not containing the gas flow of moist process gas of carbon black, P is the pressure of wet test meter, water saturation vapour pressure when being t DEG C that PW is temperature, and t is the temperature of wet test meter;
(2) calculate the water vapor that is dissolved in carbon black pregnant solution at 0 DEG C according to formula II, the condensate water volume V2Nm3 under 1 atmospheric pressure, formula II is as follows:
In formula II: the unit of V2 is Nm
3, C is the quality of carbon black pregnant solution relative to the increase of carbon black adsorption liquid, and B is the quality of dry carbon black, and 18 is the molecular weight of water, and 22.4 is 273K, under 1 atmospheric pressure, and the volume of 1mol water vapor;
(3) calculate V1 and V2 add and, obtain process gas volume to be measured.
Above-mentioned process gas volume to be measured of the present invention measure method, by first trapping in carbon black adsorption liquid by the carbon black in process gas to be measured, then wet test meter is utilized to measure the volume V of the process gas of the relatively dry after removing carbon black and most of water vapor to the moist process gas removing carbon black in process gas to be measured
1.Owing to being comprise a large amount of water vapor in process gas to be measured, this part water vapor can be condensed into water by during carbon black adsorption liquid, therefore needs additional water to be converted into the volume of water vapor under standard state, i.e. V
2.If just directly measured process gas volume to be measured before passing into carbon black adsorption liquid, so when the flow velocity of the gas by carbon black adsorption liquid is crossed slow, the just volume of not too easy accurate-metering gas to be measured, the error of measured gas volume to be measured also increases thereupon.
When computationally stating the volume of process gas to be measured, just can calculate volume in process gas to be measured shared by carbon black by the quality of carbon black divided by the density of carbon black, the volume adding shared by carbon black in the process gas volume to be measured adding and obtain of above-mentioned V1 and V2 is the cumulative volume of actual process gas to be measured.This algorithm is tighter in theory, but the quality conversion due to carbon black becomes the volume under 1 atmospheric pressure, compared with the volume of the effective process gas of the reality used in commercial production, there is the difference on the order of magnitude, even if counted in process gas cumulative volume to be measured, material alterations is not had to calculating process gas volume total amount to be measured.Therefore, the volume shared by carbon black in process gas to be measured can be ignored.
Above-mentioned process gas volume to be measured of the present invention measure method, by simple wet test meter and weighing stage, can convert and obtain the volume of process gas to be measured.The method that measures of this process gas volume to be measured of the present invention is simple, quick, accurate.
Above-mentionedly process gas to be measured to be passed in carbon black adsorption liquid of the present invention, obtain in the step of carbon black pregnant solution, the container that any container with certain capacity all can be used to hold carbon black adsorption liquid is all applicable to the present invention.In actual production process, decide to adopt the volume size of the container holding carbon black adsorption liquid according to the size of the volume of process gas to be determined, and decide according to the volume size of container the number adopting said vesse.
In a kind of preferred embodiment of the present invention, adopting is placed at least two absorption bottles by carbon black adsorption liquid respectively, and by process gas to be measured successively by each absorption bottle, collect in each absorption bottle the step of carrying out the carbon black obtained in carbon black pregnant solution after carbon black pregnant solution.By being placed on by carbon black adsorption liquid at least two absorption bottles but not an absorption bottle with twice volume, can increase the absorption number of times of carbon black on the one hand, what carbon black was adsorbed is more complete; Adopt the absorption bottle that two volumes are relatively little on the other hand, make operation more rapidly simple.
Above-mentioned process gas to be measured to be passed in carbon black adsorption liquid of the present invention, obtain in the step of carbon black pregnant solution, particular/special requirement be there is no, as long as can adsorb a certain amount of carbon black to the volume of carbon black adsorption liquid in each absorption bottle.In the present invention, the carbon black adsorption liquid in preferred each absorption bottle is not less than 10% of absorption bottle volume.When the volume that carbon black adsorption liquid accounts for absorption bottle is less than 10%, adsorbing incomplete possibility to the carbon black in a certain amount of process gas increases, and easily causes the quality of the carbon black obtained inaccurate.More preferably, by the fixing fabric structure of carbon black adsorption liquid in the scope of 10% ~ 60% of absorption bottle volume, what the carbon black in process gas to be measured can be adsorbed is more complete, the numerical value of the quality of the carbon black simultaneously obtained is unlikely to too little relative to absorption bottle and carbon black adsorption liquid gross mass, and error is also relatively little.
In a kind of specific embodiment of the present invention, above-mentionedly process gas to be measured passed in carbon black adsorption liquid, obtain in the step of carbon black pregnant solution, absorption bottle is 2 ~ 6, the volume of absorption bottle is 250ml-1000ml, and the carbon black adsorption liquid in absorption bottle is no less than 100ml.Select with 2 ~ 6 absorption bottles the carbon black in process gas to be measured can be made to adsorb more complete.Selection volume is that the absorption bottle of 250ml ~ 1000ml is convenient to observe the amount absorbing carbon black and the condensate water increased.Due to the few and particle of the amounts of carbon black of carrying secretly in process gas and small, thus in absorption bottle, carbon black adsorption liquid is preferably no less than 100ml, identical with the effect of fixing fabric structure in the scope of 10% ~ 60% of absorption bottle volume of above-mentioned carbon black adsorption liquid, also be make carbon black adsorption liquid have certain adsorptive power to process gas, and error is relatively little.
Above-mentioned process gas to be measured is passed in carbon black adsorption liquid of the present invention, obtain in the step of carbon black pregnant solution, particular/special requirement is there is no, as long as process gas to be measured can be enable by carbon black adsorption liquid and the carbon black trapped in process gas to be measured to process gas to be measured being passed into carbon black adsorption liquid level.In another preferred embodiment of the invention, process gas to be measured is passed into 1.5cm to carbon black adsorption liquid liquid level.Select the level of 1.5cm that process gas to be measured can be made all to pass in carbon black adsorption liquid in the present invention.When process gas to be measured being led to the position of below absorption liquid level close to bottom, the pressure that gas to be measured passes into carbon black adsorption liquid is larger, if it is excessively shallow that gas to be measured is more not easy to pass into liquid level quickly through carbon black adsorption liquid, the possibility that then process gas to be measured not exclusively passes in gas increases, and absorb insufficient possibility to carbon black increases thereupon.
Above-mentioned carbon black adsorption liquid of the present invention there is no particular/special requirement, as long as can adsorb carbon black and condensed steam and can not introduce other impurity and cause the inaccurate carbon black adsorption liquid of carbon black mass to be all applicable to the present invention.In the present invention, preferred carbon black adsorption liquid is water.Because aqueous phase is to pure, less on carbon black mass impact.Be more preferably ultrapure water, ultrapure water is purer, less on carbon black mass impact.
In said determination method of the present invention, process gas to be measured is passed in carbon black adsorption liquid, obtain in the step of carbon black pregnant solution, the flow velocity that process gas to be measured passes into carbon black adsorption liquid can be determined according to the relative volume of the volume of the actual process gas passed into and carbon black adsorption liquid.In the present invention, regulate process gas to be measured to pass into flow velocity in carbon black adsorption liquid, the speed making process gas to be measured produce bubble in carbon black adsorption liquid is 2 ~ 3/min.The flow control in the present invention, process gas to be measured being passed into carbon black adsorption liquid is in the scope of 2 ~ 3/min in the speed of generation bubble, and the carbon black in making process gas to be measured fully fully absorbs.Easily cause pressure in absorption bottle too large if the flow velocity passed into is too fast and absorption bottle bottle stopper is washed open.
In said determination method of the present invention, anyly carbon black in the carbon black pregnant solution obtained can be separated and the method obtaining the quality of dry carbon black is all applicable to the present invention.In one preferred embodiment of the invention, obtain the carbon black in carbon black pregnant solution, and the step measuring the quality of dry carbon black comprises: S1, get filtering material, measure the quality a of filtering material before absorbing; S2, carbon black pregnant solution to be filtered by filtering material, after drying, measure the quality b of filtering material after absorption; Difference between S3, the quality b calculating the rear filtering material of absorption and the quality a absorbing front filtering material, obtains the quality of dry carbon black.
Carbon black in above-mentioned acquisition carbon black pregnant solution of the present invention, and measure in the step of the quality of dry carbon black, by the method that carbon black pregnant solution is carried out filtering, carbon black is separated on filtering material from carbon black adsorption liquid, then drying filtering material, and by measuring filtering material filtering the quality before and after carbon black pregnant solution, the quality of carbon black enrichment fluid drying carbon black can be obtained.The method of this acquisition carbon black mass is simple, convenient and accurate.
In above-mentioned steps S1 of the present invention, get filtering material, measure in the step of the quality a of filtering material before absorbing, before any energy measurement absorbs, the method for filtering material quality is all used in the present invention.Such as, directly get dry filtering material to weigh.In the present invention, filtering material is immersed in carbon black adsorption liquid, after taking out drying, measures the quality a of filtering material before absorbing.This to measure the method for filtering material quality before absorption relatively stricter, and the difference of the quality of the carbon black after absorption carbon black pregnant solution, filter, obtained after drying is more accurate, and the quality of the carbon black obtained is more accurate.
At above-mentioned steps S2 of the present invention, carbon black pregnant solution is filtered by above-mentioned filtering material, and measure in the step of the quality b of the rear filtering material of absorption after drying, particular/special requirement be there is no to the condition of drying, as long as dry condition can be carried out by filtering the filtering material comprising carbon black obtained.In the present invention, preferred drying condition is at 105 ~ 115 DEG C, dries 2 ~ 4h.Select said temperature scope to carry out drying, the filtering material comprising carbon black and the performance not affecting filtering material can be dried.If temperature is too high, likely make filtering material character be deteriorated, carbon black also may be made to carbonize simultaneously.Drying time is controlled at 2 ~ 4h at the temperature disclosed above, the filtering material bone dry comprising carbon black can be made, and drying time again length compare and lose time.The possibility increase that the filtering material of carbon black is not exclusively dry is comprised if when being shorter than 2h, make drying time.
In said determination method of the present invention, to the amount of the filtered carbon black pregnant solution length according to required time, select Partial filtration or all filter; So in subsequent calculations process gas to be measured, during the quality of carbon black, the gross mass of the carbon black after all filtering should be calculated as.In a kind of preferred embodiment of the present invention, in above-mentioned steps S2, N/mono-getting carbon black pregnant solution cumulative volume is filtered by filtering material, measures the quality b of the rear filtering material of absorption after drying; In step S3, the quality of dry carbon black is N times of the difference between the quality b of filtering material after absorption and the quality a absorbing front filtering material.Adopt N/mono-of carbon black pregnant solution cumulative volume to carry out filtering, dry, weigh, as long as total the quality obtaining carbon black in the carbon black pregnant solution of the N/mono-volume quality of carbon black that can calculate.Get part to carry out measuring the method for weighing fast and convenient for this.
The number of times filtered by carbon black pregnant solution in above-mentioned steps S2 of the present invention is more, and that is filtered by carbon black is more complete, and the quality of the carbon black obtained is also more accurate.Correspondingly, the time of cost is also longer.In invention, preferably at least iterate through filtering material and carry out filtration step 3 times, at least carbon black just can filter more complete by filter 23 in the short period of time.More preferably 3 ~ 5 times, filter more complete 3 ~ 5 times, spended time is also relatively short.
Carbon black in the described carbon black pregnant solution of above-mentioned acquisition of the present invention, and measure in the step of the quality of dry carbon black, the filtering material used there is no particular/special requirement, as long as can by the carbon black isolated by filtration in carbon black pregnant solution out.In the present invention, preferred filtering material is included in the filter paper filtering and first contact with carbon black pregnant solution in carbon black pregnant solution process, and is positioned at the acid-washed asbestos below filter paper.Adopt filter paper and the acid-washed asbestos below it to coordinate to use as filtering material, to carbon black, there is higher filtration efficiency.More preferably filter paper is quantitative filter paper.Need the carbon black stayed on filter paper to weigh together with after filter paper drying after filtering carbon black pregnant solution in the present invention, and the ash content quality after quantitative filter paper ashing is a definite value, analysis result is not had an impact substantially, is applicable to the mass method analysis design mothod in chemical analysis.
In above-mentioned filtration step of the present invention, anyly all can be applicable to the present invention with the filtration utensil that above-mentioned filtering material carries out filtering, particular/special requirement be there is no to the concrete specification of filtering utensil.In one preferred embodiment of the invention, filtering material is placed in Buchner funnel or glass sand core funnel filters, the internal diameter of preferred Buchner funnel or glass sand core funnel is not more than 10cm; Meanwhile, the diameter being preferably placed at filter paper in Buchner funnel or glass sand core funnel and acid-washed asbestos is not more than 11cm.Buchner funnel or glass sand core funnel are the filtration utensils that laboratory is commonly used, and compare common funnel, can connect aspiration pump and carry out suction filtration to accelerate filter velocity, shorten analysis time.The relatively little ratio of density of carbon black pregnant solution to be filtered in the present invention is easier to suction filtration, adopts diameter to be not more than the Buchner funnel of 10cm or glass sand core funnel just can complete filtration step very like a cork.Be greater than Buchner funnel or the glass sand core funnel of 10cm according to diameter, filter velocity can be made faster, but due to carbon black pregnant solution and the corresponding increase of contact area of the filtering material in Buchner funnel or glass sand core funnel, error increase relatively.Select diameter be not more than the filter paper of 11cm and acid-washed asbestos be make itself and corresponding Buchner funnel or sand core funnel with the use of.
Said determination method of the present invention has been enough to the content of carbon black in process gas to be measured, but in order to remove the sour gas contained in process gas to be measured further, to prevent the corrosive attack when measuring process gas volume to be measured to gauging instrument, before the moist process gas not containing carbon black is passed into wet test meter by above-mentioned steps of the present invention (1), also comprise the step of moist process gas by alkaline solution absorption sour gas by not containing carbon black.
In the step of above-mentioned removal sour gas, select alkaline solution to absorb the sour gas in moist process gas, sour gas can be absorbed well by acid-base neutralization.The alkaline solution of any sour gas that can be diluted in moist process gas by above-mentioned acid-base neutralization is all applicable to the present invention, only otherwise cause subsequent instrumentation and corrode.Preferred alkaline solution is NaOH, KOH, NaHCO3 or KHCO3 solution.To the mass concentration of alkaline solution used also without particular/special requirement, equally, as long as can it be made not cause subsequent instrumentation corrode by the sour gas absorbed in moist process gas.In the present invention, be preferably the alkaline solution of 0.3 ~ 0.8% by mass concentration, the alkaline solution of mass concentration within the scope of this can utilize less energy consumption enough to absorb sour gas in moist process gas, make it be not easy to cause corrosion to follow-up instrument, more preferably mass concentration is the alkaline solution of 0.5%.
In said determination method of the present invention, when the ammonia level in process gas to be measured is larger, after the step absorbing sour gas, the step of removing ammonia is also set further, removes ammonia to prevent from causing corrosion to instrument.In a kind of preferred embodiment of the present invention, before the moist process gas not containing carbon black is passed into wet test meter by above-mentioned steps (1), further comprise and the moist process gas removing sour gas is passed into the CaCl that mass concentration is 0.3-0.8%
2solution absorbs the step of ammonia, preferred CaCl
2solution to be mass concentration be 0.5% CaCl
2solution.
In the step of above-mentioned removing ammonia of the present invention, adopt weakly acidic CaCl
2if solution absorbs the ammonia of alkalescence by neutralization reaction.Work as CaCl
2when the mass concentration of solution is in 0.3 ~ 0.8% scope, just can more fully absorb foreign gas ammonia, when mass concentration is 0.5%, better to the assimilation effect of ammonia.
The assay method of content of carbon black in process gas provided by the present invention, had both been applicable to the mensuration of content of carbon black in this process gas of water gas, had also been applicable to the mensuration of content of carbon black in flue gas.
Beneficial effect of the present invention is further illustrated below in conjunction with specific embodiment.
Reagent used in the following example and instrument as follows:
Absorption bottle (250ml, 500ml, 1000ml tri-kinds of capacity)
Wet test meter 1
Analytical balance one (precision: 0.0001g)
Buchner funnel (or glass sand core funnel, ￠ 100cm) 1
Bottle,suction
Wash bottle (500ml)
Thermostatic drying chamber 1
Quantitative filter paper (￠ 11cm)
Embodiment 1
One, preliminary work:
(1) to try to please two absorption bottles amassed as 250ml, in absorption bottle 1 and absorption bottle 2, be respectively charged into 100ml high purity water, after weighing, be C1, draft tube is inserted below water surface 1.5cm, absorption bottle and draft tube pipe are carried into process gas scene and sample.
(2) with ultrapure water, acid-washed asbestos and filter paper are infiltrated in advance, then baking oven put into by the related Buchner funnel holding acid-washed asbestos and filter paper, at 105 DEG C of dry 3h, in exsiccator after cooling, quick and precisely take the quality a absorbing front dry Buchner funnel (together with acid-washed asbestos and filter paper) with analytical balance.
(3) to volume be 250nl absorption bottle 3 in fill the NaOH solution that 100ml mass concentration is 0.5%, be carried into sampling on-the-spot for subsequent use.
(4) to volume be 250nl absorption bottle 4 in fill the CaCl that 100ml mass concentration is 0.5%
2solution, is carried into sampling on-the-spot for subsequent use.
Two, sample
According to flow process shown in accompanying drawing 1, the stopple coupon with flow control valve is connected with absorption bottle 2 with absorption bottle 1, is measured by wet test meter from absorption bottle 2 gas out.On-the-spot in sampling, slightly open sample valve, sweep sampling line with the air-blowing of water gas sample, then in adjust flux to absorption bottle 1 and absorption bottle 2, the speed of bubble is 2 bubbles p.s., and the gas flow A read by wet test meter is 150Nm
3, the site environment atmospheric pressure P that wet test meter is measured is 101.4MPa, and the temperature t that wet test meter is measured is 27 DEG C; When temperature t is 27 DEG C, water saturation vapour pressure PW is 35.67mBa.
After sampling terminates, take absorption bottle 1 and absorption bottle 2 with analytical balance and absorb quality C2 in water gas after carbon black and condensate water, and C2 is deducted the quality that C1 gained difference C is the increase in absorption bottle 1 and absorption bottle 2 planar water coal gas after carbon black and condensate water.
Three, separating off carbon black
The filtering flask of known quality is placed in filtration on bottle,suction and is enriched with the absorption bottle 1 of carbon black and whole water samples of absorption bottle 2, filter 23.
After filtration terminates, Buchner funnel (together with filter paper and acid-washed asbestos) is put into baking oven, dry 3 hours at 105 DEG C, in exsiccator after cooling, quick and precisely take the quality b absorbing rear dry Buchner funnel (together with acid-washed asbestos and filter paper) with analytical balance.
Four, the calculating of content of carbon black
According to formula I
calculate 0 DEG C, the volume V1Nm of process gas dry under 1 atmospheric pressure
3;
According to formula II
calculate the water vapor that is dissolved in described carbon black pregnant solution at 0 DEG C, the condensate water volume V under 1 atmospheric pressure
2nm
3;
Finally, according to formula III
calculate content of carbon black in water gas to be measured, result of calculation is in table 1.
Embodiment 2
One, preliminary work:
(1) to try to please long-pending 4 absorption bottles being 500ml, 200ml tap water is filled in absorption bottle 1, absorption bottle 2, absorption bottle 3 and absorption bottle 4, four absorption bottles weigh after gross mass be designated as C1, draft tube is inserted below water surface 2cm, and absorption bottle 1, absorption bottle 2, absorption bottle 3 and absorption bottle 4 and draft tube are carried into process gas scene sample.
(2) with tap water, acid-washed asbestos and filter paper are infiltrated in advance, then the related glass sand core funnel holding acid-washed asbestos and filter paper puts into baking oven, at 115 DEG C of dry 3h, in exsiccator after cooling, quick and precisely take the quality a absorbing front dry Buchner funnel (together with acid-washed asbestos and filter paper) with analytical balance.
(3) to volume be 500ml absorption bottle 5 in fill the NaOH solution that 150ml mass concentration is 0.3%, be carried into sampling on-the-spot for subsequent use.
(4) to volume be 500ml absorption bottle 6 in fill the CaCl that 150ml mass concentration is 0.3%
2solution, is carried into sampling on-the-spot for subsequent use.
Two, sample
According to flow process shown in accompanying drawing 1, the stopple coupon with flow control valve is connected with absorption bottle 4 with absorption bottle 1, absorption bottle 2, absorption bottle 3, is measured by wet test meter from absorption bottle 4 gas out.On-the-spot in sampling, slightly open sample valve, sweep sampling line with the air-blowing of water gas sample, then in adjust flux to absorption bottle 1, absorption bottle 2, absorption bottle 3 and absorption bottle 4, the speed of bubble is 2 bubbles per second, and the gas flow A read by wet test meter is 130Nm
3, the site environment atmospheric pressure P that wet test meter is measured is 101.4MPa, and the temperature t that wet test meter is measured is 27 DEG C; When temperature t is 27 DEG C, water saturation vapour pressure PW is 35.67mBa.
After sampling terminates, take absorption bottle 1, absorption bottle 2, absorption bottle 3 and absorption bottle 4 with analytical balance and absorb quality C2 in water gas after carbon black and condensate water, and C2 is deducted C1 gained difference C and be the quality that absorption bottle 1, absorption bottle 2, absorption bottle 3 and absorption bottle 4 absorb the increase in water gas after carbon black and condensate water, meanwhile, the quality that absorption bottle 1 absorbs in water gas after carbon black and condensate water accounts for 1/2 of gross mass C2.
Three, separating off carbon black
The filtering flask of known quality is placed in filtration on bottle,suction and is enriched with the absorption bottle 1 of carbon black and whole water samples of absorption bottle 2, filter 4 times.
After filtration terminates, Buchner funnel (together with filter paper and acid-washed asbestos) is put into baking oven, dry 2 hours at 115 DEG C, in exsiccator after cooling, quick and precisely take the quality b absorbing rear dry Buchner funnel (together with acid-washed asbestos and filter paper) with analytical balance.
Four, the calculating of content of carbon black
According to formula I
calculate 0 DEG C, the volume V1Nm of process gas dry under 1 atmospheric pressure
3;
According to formula II
calculate the water vapor that is dissolved in described carbon black pregnant solution at 0 DEG C, the condensate water volume V under 1 atmospheric pressure
2nm
3; B=2* (b-a)
Finally, according to formula III
calculate content of carbon black in water gas to be measured, result of calculation is in table 1.
Embodiment 3
One, preliminary work:
(1) be in the absorption bottle 1 of 1000ml, absorption bottle 2 and absorption bottle 3 to volume and fill 100ml high purity water, postscript of weighing is C1, draft tube is inserted below water surface 1.5cm, and absorption bottle 1, absorption bottle 2, absorption bottle 3 and draft tube are carried into process gas scene sample.
(2) with tap water, acid-washed asbestos and filter paper are infiltrated in advance, then the related glass sand core funnel holding acid-washed asbestos and filter paper puts into baking oven, at 110 DEG C of dry 3h, in exsiccator after cooling, quick and precisely take the quality a absorbing front dry Buchner funnel (together with acid-washed asbestos and filter paper) with analytical balance.
(3) to volume be 1000ml absorption bottle 4 in fill the NaOH solution that 200ml mass concentration is 0.8%, be carried into sampling on-the-spot for subsequent use.
(4) to volume be 1000ml absorption bottle 5 in fill the CaCl that 200ml mass concentration is 0.8%
2solution, is carried into sampling on-the-spot for subsequent use.
Two, sample
Shown in accompanying drawing 1, the stopple coupon with flow control valve is connected with absorption bottle 3 with absorption bottle 1, absorption bottle 2, is measured by wet test meter from absorption bottle 3 gas out.On-the-spot in sampling, slightly open sample valve, sweep sampling line with the air-blowing of water gas sample, then in adjust flux to absorption bottle 1, absorption bottle 2 and absorption bottle 3, the speed of bubble is 2 bubbles p.s., and the gas flow A read by wet test meter is 150Nm
3, the site environment atmospheric pressure P that wet test meter is measured is 101.4MPa, and the temperature t that wet test meter is measured is 27 DEG C; When temperature t is 27 DEG C, water saturation vapour pressure PW is 35.67mBa.
After sampling terminates, take absorption bottle 1, absorption bottle 2 and absorption bottle 3 with analytical balance and absorb quality C2 in flue gas after carbon black and condensate water, and C2 being deducted the quality that C1 gained difference C is the increase in absorption bottle 1 and absorption bottle 2 planar water coal gas after carbon black and condensate water, the quality that absorption bottle 1 and absorption bottle 2 absorb in water gas after carbon black and condensate water accounts for 1/3 of gross mass C2.
Three, separating off carbon black
The filtering flask of known quality is placed in filtration on bottle,suction and is enriched with the absorption bottle 1 of carbon black and whole water samples of absorption bottle 2, filter 6 times.
After filtration terminates, Buchner funnel (together with filter paper and acid-washed asbestos) is put into baking oven, dry 4 hours at 110 DEG C, in exsiccator after cooling, quick and precisely take the quality b absorbing rear dry Buchner funnel (together with acid-washed asbestos and filter paper) with analytical balance.
Four, the calculating of content of carbon black
According to formula I
calculate 0 DEG C, the volume V1Nm of process gas dry under 1 atmospheric pressure
3;
According to formula II
calculate the water vapor that is dissolved in described carbon black pregnant solution at 0 DEG C, the condensate water volume V under 1 atmospheric pressure
2nm
3; B=3* (b-a)
Finally, according to formula III
calculate content of carbon black in water gas to be measured, result of calculation is in table 1.
Embodiment 4
One, preliminary work:
(1) be in the absorption bottle 1 of 250ml and absorption bottle 2 to volume and fill 100ml high purity water, draft tube is inserted below water surface 1.5cm, absorption bottle and draft tube are carried into process gas scene and sample.
(2) with ultrapure water, acid-washed asbestos and filter paper are infiltrated in advance, then baking oven put into by the related Buchner funnel holding acid-washed asbestos and filter paper, at 105 DEG C of dry 3h, in exsiccator after cooling, quick and precisely take the quality a absorbing front dry Buchner funnel (together with acid-washed asbestos and filter paper) with analytical balance.
(3) to volume be 250nl absorption bottle 3 in fill the NaOH solution that 100ml mass concentration is 0.5%, be carried into sampling on-the-spot for subsequent use.
(4) to volume be 250nl absorption bottle 4 in fill the CaCl that 100ml mass concentration is 0.5%
2solution, is carried into sampling on-the-spot for subsequent use.
Two, sample
Connect slightly different from the device of embodiment 1, pipeline between variable valve and absorption bottle is provided with electronic gas flowmeter, being arranged by variable valve makes flowmeter display instantaneous delivery be stabilized in 10ml/s, controls sampling time and flow velocity, can obtain the volume of sample gas as calculated.On-the-spot in sampling, slightly open sample valve, sweep sampling line with the air-blowing of water gas sample, then in adjust flux to absorption bottle 1 and absorption bottle 2, the speed of bubble is 2 bubbles p.s., and sampling 3h, as calculated, the cumulative volume of gained process gas is 108Nm
3.
After sampling terminates, the absorption bottle 1 after carbon black in absorption water gas and condensate water and absorption bottle 2 are taken back laboratory and carries out carbon black lock out operation.
Three, separating off carbon black
The filtering flask of known quality is placed in filtration on bottle,suction and is enriched with the absorption bottle 1 of carbon black and whole water samples of absorption bottle 2, filter 23.
After filtration terminates, Buchner funnel (together with filter paper and acid-washed asbestos) is put into baking oven, dry 3 hours at 105 DEG C, in exsiccator after cooling, quick and precisely take the quality b absorbing rear dry Buchner funnel (together with acid-washed asbestos and filter paper) with analytical balance.
Four, the calculating of content of carbon black
According to formula
calculate content of carbon black in water gas to be measured, result of calculation is in table 1.
Embodiment 5,6,7 is that to detect the repeatability of this assay method, the measurement result of content of carbon black is in table 2 according to the step described in embodiment 1 by the content of carbon black replication in water gas to be measured three times.
Table 1
Table 2
As can be seen from Table 1, the above embodiments of the present invention, by trapping in water by the carbon black carried secretly in process gas, measure the volume of process gas with wet test meter, then to filtering and the dry carbon black trapped, oven dry is weighed, and then obtains the content of carbon black in process gas.The advantage of the method is the trapping work that directly can complete carbon black at the scene, in laboratory, complete filtration, the dry and work that weighs, the assay method of content of carbon black in process gas is become simply, fast, accurate.Due to the present invention's employing is mass method, and error is also less.The experiment that three time repeat of this point from table 2 also can be found out, the relative deviation that in table 2, three times measure all is less than 3%, and therefore, assay method of the present invention is reproducible, and accuracy is also higher.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (14)
1. the assay method of content of carbon black in process gas, it is characterized in that, this assay method comprises the following steps:
Get the process gas containing carbon black, form process gas to be measured;
Described process gas to be measured is passed in carbon black adsorption liquid, obtains carbon black pregnant solution and not containing the moist process gas of carbon black;
Obtain the carbon black in described carbon black pregnant solution, and weigh the quality of dry carbon black;
Calculate the ratio between the quality of described dry carbon black and the volume of described process gas to be measured, obtain the content of carbon black in described process gas.
2. assay method according to claim 1, is characterized in that, the volume of described process gas to be measured is calculated by following steps:
(1) the moist process gas not containing carbon black is passed into wet test meter, calculate 0 DEG C according to formula I, the volume V of process gas dry under 1 atmospheric pressure
1, described formula I is as follows:
In formula I: V
1unit be Nm
3, A is the gas flow not containing the moist process gas of carbon black by wet test meter, and P is the pressure of wet test meter, P
wfor water saturation vapour pressure when temperature is t DEG C, t is the temperature value that wet test meter reads;
(2) water vapor that is dissolved in described carbon black pregnant solution is calculated at 0 DEG C according to formula II, the condensate water volume V under 1 atmospheric pressure
2, described formula II is as follows:
In formula II: V
2unit be Nm
3, C is the quality of described carbon black pregnant solution relative to the increasing of described carbon black adsorption liquid, and B is the quality of described dry carbon black, and 18 is the molecular weight of water, and 22.4 is 273K, under 1 atmospheric pressure, and the volume of 1mol water vapor;
(3) calculate V1 and V2 add and, obtain described process gas volume to be measured.
3. assay method according to claim 1 and 2, it is characterized in that, described process gas to be measured is passed in carbon black adsorption liquid, obtain in the step of carbon black pregnant solution, carbon black adsorption liquid is placed on respectively at least two absorption bottles, and by described process gas to be measured successively by each described absorption bottle, collect the step of carrying out the carbon black obtained in described carbon black pregnant solution in each absorption bottle after carbon black pregnant solution.
4. assay method according to claim 3, is characterized in that, described in each described absorption bottle, the volume of carbon black adsorption liquid is not less than 10% of described absorption bottle volume, and described process gas passes into 1.5cm to described carbon black adsorption liquid liquid level; Preferably, described absorption bottle is 2 ~ 6, and the volume of described absorption bottle is 250ml-1000ml, and the carbon black adsorption liquid in described absorption bottle is no less than 100ml; Preferred described carbon black adsorption liquid is water, is more preferably ultrapure water.
5. assay method according to claim 1 and 2, it is characterized in that, described process gas to be measured is passed in carbon black adsorption liquid, obtain in the step of carbon black pregnant solution, regulate described process gas to be measured to pass into flow velocity in carbon black adsorption liquid, the speed making described process gas to be measured produce bubble in carbon black adsorption liquid is 2 ~ 3/min.
6. assay method according to claim 1 and 2, is characterized in that, obtain the carbon black in described carbon black pregnant solution, and the step measuring the quality of dry carbon black comprises:
S1, get filtering material, measure the quality a of filtering material before absorbing;
S2, described carbon black pregnant solution to be filtered by described filtering material, after drying, measure the quality b of filtering material after absorption;
Difference between S3, the quality b calculating the rear filtering material of absorption and the quality a absorbing front filtering material, obtains the quality of described dry carbon black.
7. assay method according to claim 6, is characterized in that, in described step S1, gets filtering material, is immersed in by described filtering material in described carbon black adsorption liquid, takes out after drying, measures the quality a of filtering material before described absorption.
8. assay method according to claim 6, is characterized in that, in described step S2, drying condition is at 105 ~ 115 DEG C, dries 2 ~ 4h.
9. assay method according to claim 6, is characterized in that,
In described step S2, N/mono-getting described carbon black pregnant solution cumulative volume is filtered by described filtering material, measures the quality b of the rear filtering material of absorption after drying;
In described step S3, the quality of described dry carbon black be the N of difference between the quality a of filtering material before the quality b of filtering material after described absorption and described absorption doubly.
10. assay method according to claim 6, is characterized in that, in described step S2, described carbon black pregnant solution is at least iterated through described filtering material and carries out described filtration step 3 times, preferably 3 ~ 5 times.
11. assay methods according to claim 6, is characterized in that, described filtering material is included in the filter paper filtering and first contact with described carbon black pregnant solution in described carbon black pregnant solution process, and is positioned at the acid-washed asbestos below described filter paper; Preferred described filter paper is quantitative filter paper.
12. assay methods according to claim 11, is characterized in that, in described filtration step, described filtering material are placed in Buchner funnel or glass sand core funnel filters, and the diameter of preferred described Buchner funnel or glass sand core funnel is not more than 100cm; The diameter of the described filter paper and acid-washed asbestos that are more preferably arranged in described Buchner funnel or glass sand core funnel is not more than 11cm.
13. assay methods according to claim 2, it is characterized in that, described step (1) by before not passing into wet test meter containing the moist process gas of carbon black, also comprise by described not containing the moist process gas of carbon black by alkaline solution to absorb the step of the sour gas in described moist process gas; Preferred described alkaline solution to be mass concentration be 0.3 ~ 0.8% alkaline solution, more preferably mass concentration is the alkaline solution of 0.5%; Preferred described alkaline solution is NaOH, KOH, NaHCO
3or KHCO
3solution.
14. assay methods according to claim 13, it is characterized in that, after the step of described absorption sour gas, described step (1) further comprises and passes into removing the moist process gas after sour gas the CaCl that mass concentration is 0.3 ~ 0.8% before the moist process gas not containing carbon black is passed into wet test meter
2solution to absorb the step of ammonia, preferred described CaCl
2solution to be mass concentration be 0.5% CaCl
2solution.
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Address after: 100011 Beijing Dongcheng District, West Binhe Road, No. 22 Patentee after: China Shenhua Energy Co.,Ltd. Patentee after: Guoneng Baotou Coal Chemical Co.,Ltd. Patentee after: CHINA SHENHUA COAL TO LIQUID AND CHEMICAL Co.,Ltd. Address before: 100011 Beijing Dongcheng District, West Binhe Road, No. 22 Patentee before: China Shenhua Energy Co.,Ltd. Patentee before: SHENHUA BAOTOU COAL CHEMICAL Co.,Ltd. Patentee before: CHINA SHENHUA COAL TO LIQUID AND CHEMICAL Co.,Ltd. |